高效液相法测定陈皮药渣中橙皮苷含量

摘 要 目的:通过对陈皮药材及药渣中橙皮苷含量进行比较分析,为陈皮药渣的二次开发提供依据。方法: 色谱柱:Eclipse XDB- C₁₈(280 mm×4.6 mm, 5 μm)流动相：甲醇∶水∶冰醋酸（30∶66∶4）;流速：1.0 ml·min^-1;检测波长：283 nm。结果:橙皮苷与其它色谱峰分离良好。橙皮苷的线性范围在0.42～4.20 μg,r=0.999 7。陈皮药材的平均加样回收率为98.5%,RSD=2.12%(n=6);陈皮药渣的平均加样回收率为98.1%,RSD=2.35%(n=6)。结论:陈皮药渣中橙皮苷的提取量为陈皮药材中橙皮苷的提取量52%,表明陈皮药渣具有二次开发利用的价值。     

HPLC法测定大青龙汤颗粒剂中盐酸麻黄碱和盐酸伪麻黄碱的含量

摘 要 目的:建立HPLC测定大青龙汤颗粒剂中盐酸麻黄碱和盐酸伪麻黄碱含量的方法,为该制剂的质量控制提供依据。方法: 采用Agilent Zorbax SB-C₁₈色谱柱(150 mm×4.6 mm,5 μm),以乙腈-含0.3%三乙胺的0.02 mol·L^-1磷酸二氢钾溶液（用磷酸调节至pH=3.0）(5∶95)为流动相,流速:1.0 ml·min^-1,波长：207 nm。结果:盐酸麻黄碱在64～640 μg·ml^-1浓度范围内线性关系良好（r=0.999 6）,平均回收率为101.66%,RSD为2.59%(n=6);盐酸伪麻黄碱在31.8～318 μg·ml^-1浓度范围内呈现良好的线性关系（r=0.999 7）,平均回收率为99.70%,RSD为1.58%(n=6)。结论:该法简便易行,结果准确,可用于大青龙汤颗粒剂的质量控制。     

HPLC法测定妥布霉素滴眼液中5种抑菌剂

目的 建立同时测定妥布霉素滴眼液中5种抑菌剂(羟苯乙酯、硫柳汞、羟苯丙酯、苯扎溴铵和苯扎氯铵)的HPLC方法。方法 采用Agilent Zorbax SB-C₁₈ (4.6 mm×150 mm,5 μm)色谱柱,流动相A为1%三乙胺（磷酸调节pH值至3.5±0.05）;流动相B为甲醇,梯度洗脱,流速为1.0 mL·min^-1,柱温35 ℃,检测波长为214 nm。结果 羟苯乙酯、硫柳汞、羟苯丙酯、苯扎溴铵/苯扎氯铵各峰均分离良好;羟苯乙酯在0.77～192.5 μg·mL-1范围内线性关系良好(r=0.999 5),平均回收率为100.0%(RSD=0.9%,n=9);硫柳汞在2.16～541.0 μg·mL^-1范围内线性关系良好(r=0.999 7),平均回收率为100.1%(RSD=0.6%,n=9);羟苯丙酯在0.84～209.8 μg·mL^-1范围内线性关系良好(r=1.000 0),平均回收率为100.3%(RSD=1.0%,n=9);苯扎溴铵在4.36～1090 μg·mL^-1范围内线性关系良好(r=0.9992),平均回收率为100.2%(RSD=0.5%,n=9);苯扎氯铵（n-C12H25）3.22～805.0 μg·mL^-1范围内线性关系良好(r=0.999 8),平均回收率为100.1%(RSD=1.1%,n=9);苯扎氯铵（n-C14H29）1.66～413.9 μg·mL^-1范围内线性关系良好(r=1.000 0),平均回收率为100.1%(RSD=0.6%,n=9)。结论 该方法准确、灵敏、简便,可用于妥布霉素滴眼液中羟苯乙酯、硫柳汞、羟丙丙酯、苯扎溴铵及苯扎氯铵5种抑菌剂的检查。     

黄芪饮片中4个异黄酮类成分的含量测定

摘 要 目的:建立高效液相色谱法测定黄芪饮片中4个异黄酮成分的含量方法。方法: 色谱柱为Agilent Zorbax SB-C₁₈(250 mm×4.6 mm,5 μm) ,流动相为乙腈-水梯度洗脱,流速1.0 ml·min^-1,检测波长为260 nm, 柱温30℃,进样量10 μl。结果:毛蕊异黄酮-7-葡萄糖苷、芒柄花苷、毛蕊异黄酮、芒柄花素分别在4.42～442 μg·ml^-1、2.06～206 μg·ml^-1、3.36～336 μg·ml^-1、4.60～460 μg·ml^-1浓度范围内与各自峰面积积分值呈良好的线性关系;平均回收率分别为99.4%(RSD=5.34%)、94.8%(RSD=2.39%)、98.9%(RSD=3.69%)、102.3%(RSD=3.01%)(n=9)。结论:本方法简便、准确、重复性好,可用于黄芪饮片的质量控制。     

HPLC同时测定半夏糖浆中琥珀酸、橙皮苷、甘草苷3种成分的含量

目的 建立HPLC同时测定半夏糖浆中琥珀酸、橙皮苷、甘草苷3种成分的含量。方法 采用C₁₈色谱柱（4.6 mm×150 mm,5μm）,以乙腈-0.2%磷酸溶液（18：82）为流动相,流速1.0 mL·min^-1,检测波长207 nm,柱温为常温。结果 3种待测成分分离度良好,阴性无干扰;3个成分线性范围分别为4.727~118.17 μg·mL^-1（r=0.999 9）,2.474~61.857 μg·mL^-1（r=0.999 6）,2.469~61.725 μg·mL^-1（r=0.999 9）;琥珀酸、橙皮苷、甘草苷平均回收率（n=9）分别为100.8%,99.3%,100.2%,RSD分别为1.3%,1.2%,1.8%,3批中琥珀酸、橙皮苷、甘草苷含量范围分别为0.072 2~0.079 4、0.029 9~0.034 8,0.022 8~0.029 0 mg·mL^-1。结论 该方法操作简单,缩短了分析时间,重复性好,可为半夏糖浆质量控制提供参考。     

HPLC法测定妇安消疹洗液中苦参碱与氧化苦参碱的含量

摘 要 目的:建立测定妇安消疹洗液中苦参碱与氧化苦参碱含量的高效液相色谱(HPLC)方法。方法: 采用Inertsil NH₂(250 mm×4.6 mm,5 μm) 色谱柱;流动相为乙腈-无水乙醇-3%磷酸溶液(80∶10∶10),流速为1.0 ml·min^-1,检测波长220 nm。结果:苦参碱与氧化苦参碱分别在0.048 9～0.978 0 mg·ml^-1(r=0.999 9)与0.053 5～1.070 0 mg·ml^-1(r=0.999 9)范围内线性关系良好,平均回收率分别为98.72%与99.49%,RSD分别为1.60%与1.23%。结论:该方法简单,结果准确、可靠,可用于妇安消疹洗液的质量控制。     

HPLC法同时测定复方三维右旋泛酸钙糖浆中4中维生素的含量

目的 建立高效液相色谱(HPLC)法同时测定复方三维右旋泛酸钙糖浆中维生素B₁、维生素B₂、维生素B₆和烟酰胺的含量。方法 采用外标法进行测定,色谱柱为Thermo Betasil C₁₈ Analytical(4.6 mm×250 mm, 5 μm),流动相为乙腈-5 mmol·L^-1十二烷基硫酸钠（含0.05%甲酸）水溶液梯度洗脱,流速1.0 mL·min^-1,检测波长260 nm,柱温30 ℃。分别测定10批复方三维右旋泛酸钙糖浆。结果 维生素B₁、维生素B₂、维生素B₆、烟酰胺4种成分的线性范围分别为5.76~115.2 μg·mL^-1(r=0.999 9)、1.16~23.20 μg·mL^-1(r=0.999 9)、1.72~34.4 μg·mL^-1(r=0.999 6)和5.76~115.2 μg·mL^-1(r=0.999 9),平均加样回收率为96.2%~98.4%(RSD为2.14%~3.42%)。不同批次复方三维右旋泛酸钙糖浆中维生素B₁、维生素B₂、维生素B₆、烟酰胺含量范围分别为0.133 7~0.155 9、0.027 86~0.030 71、0.039 05~0.047 7、0.138 7~0.148 2 mg·g^-1。结论 该方法为完善复方三维右旋泛酸钙糖浆的质量标准和加强质量控制提供了新的方法和依据。     

高灵敏度HPLC测定大鼠血浆中益母草碱浓度及其药动学研究

目的 建立一种高灵敏度HPLC测定大鼠血浆中益母草碱浓度,并研究益母草碱在大鼠体内的药动学特征。方法 大鼠口服益母草碱混悬溶液（50 mg·kg^-1）后,不同时间点尾静脉采血,以苯甲酰精氨酸乙酯为内标,血浆样品经酸化后乙酸乙酯萃取,采用HPLC进行测定。色谱条件：采用Diamonsil C₁₈（250 mm×4.6 mm,5 μm）为色谱柱,以乙腈-0.02 mol·L^-1磷酸二氢钾缓冲溶液（pH 3.0）（22：78）为流动相,流速1.0 mL·min^-1,柱温35℃,检测波长277 nm。并利用PKS 1.0软件计算药动学参数。结果 益母草碱血浆浓度在0.05~1.5 μg·mL^-1内线性关系良好（r=0.999 1）。方法的定量下限（LLOQ）为0.05 μg·mL^-1（RSD=12.8%,n=5）;提取回收率为76.5%~82.5%;批内、批间准确度为96.9%~104.9%;日内、日间精密度均<10%;质控样品经反复冻融3次及-20℃放置1个月后均较稳定。大鼠口服益母草碱后,药-时曲线符合二室开放模型,主要药动学参数为t_max=0.95 h,C_max=0.51 μg·mL^-1,t_1/2=3.64 h,AUC_0-t=1.56 μg·mL^-1·h^-1,AUC_0-∞=1.78 μg·mL^-1·h^-1。结论 该方法准确度、灵敏度高,重复性好,可用于生物样品中益母草碱浓度的测定。     

柱前衍生-HPLC测定白消安在家兔体内的药动学参数

目的 建立测定家兔血清中白消安浓度和家兔体内药动学特征的柱前衍生化HPLC。方法 以1,5-戊二醇二甲磺酸酯为内标,二乙基二硫代氨基甲酸钠为衍生化试剂。流动相：甲醇-水（54∶46）,流速：0~20 min（1.0 mL·min^-1）,20~27 min（1.3 mL·min^-1）。柱温：30℃,检测波长：280 nm,进样量：25 μL。家兔分别以灌胃、静注的方式给予白消安,按本法测定血药浓度,DAS 3.0计算药动学参数。结果 白消安的血药浓度在0.1~3.4 mg·-L¹ 内线性关系良好（r=0.999 7）,日内、日间精密度以及样品稳定性符合中国药典2015年版的规定。低、中、高浓度的萃取回收率分别为90.0%,89.0%,91.5%。不同给药途径获得的药动学参数：单剂量口服t_1/2=（2.26±0.66）h,k=（0.33±0.12）·h^-1,k_a=（2.54±1.3）·h^-1,AUC_0–t=（1.95±0.18）h·mg·mL^-1;单剂量静脉注射t_1/2=（1.53±0.09）h,k=（0.45±0.03）·h^-1,AUC_0–∞=（4.38±0.26）h·mg·mL^-1。多剂量口服后C_ss=（0.48±0.03）mg·mL^-1,AUC_0–τ=（3.87±0.26）h·mg·mL^-1。结论 建立的柱前衍生-HPLC法适用于白消安血药浓度测定及药动学研究,不同给药途径的药动学参数为临床药动学研究提供了依据。     

邻苯二甲醛柱前衍生化-HPLC测定复方氨基酸注射液中蛋氨酸亚砜的含量

目的 建立测定复方氨基酸注射液中蛋氨酸亚砜含量的方法。方法 采用邻苯二甲醛（O-phthaladehyde,OPA）柱前衍生HPLC。色谱柱为Agilent ZORBAX Eclipse AAA C₁₈柱（150 mm×4.6 mm,5µm）,检测波长为338 nm,流动相A为0.04 mol·L^-1磷酸二氢钠溶液（调节pH至7.8）,流动相B为乙腈-甲醇-水（45：45：10）,梯度洗脱,流速为2.0 ml·min^-1,柱温为40℃,供试品溶液与OPA衍生剂及硼酸盐缓冲液按设定程序自动混匀后进样。结果 蛋氨酸亚砜的质量浓度线性范围为0.000 5~0.050 0 mg·mL^-1（R=0.999 9）;定量限为0.250 5 μg·mL^-1,检测限为0.083 5 μg·mL^-1;精密度、稳定性、重复性试验的RSD<3.0%;平均回收率为99.1%（RSD=1.33%,n=9）。结论 该方法操作简便,可用于复方氨基酸注射液中蛋氨酸亚砜的含量测定。     

Efficacy of gut lavage,hemodialysis, and hemoperfusion in the therapy of paraquat or diquat intoxication

Clinical and in vitro investigations were carried out to test the efficacy of gut lavage, hemodialysis, and hemoperfusion in the treatment of poisoning with paraquat or diquat. In a patient suffering from diquat intoxication 130 times more diquat was removed by gut lavage 30 h after ingestion than was removed by complete aspiration of the gastric contents.Determination of in vitro clearances for paraquat and diquat by hemodialysis showed that, at serum concentrations of 1–2 ppm, such as are frequently encountered in poisoning in man, toxicologically relevant quantities of herbicide cannot be removed from the body. At a concentration of 20 ppm, on the other hand, hemodialysis proved to be effective, the clearance being 70 ml/min at a blood flow rate of 100 ml/min. The efficacy of hemoperfusion with coated activated charcoal was on the whole better. Especially at concentrations around 1–2 ppm, the clearance values for hemoperfusion were some 5–7 times higher than those for hemodialysis.In a patient suffering from paraquat poisoning, both hemodialysis as well as hemoperfusion were carried out. The in vitro results could be confirmed: At serum concentrations of paraquat less than 1 ppm no clearance could be obtained by hemodialysis while by hemoperfusion with activated charcoal quite high clearance values were measured and the serum level dropped down to zero.

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Zusammenfassung Klinische Untersuchungen und Laboratoriumsversuche wurden durchgeführt, um die Wirksamkeit von Darmspülung, Hämodialyse und Hämoperfusion bei Paraquat- und Deiquat-Vergiftungen zu prüfen.Bei einem Patienten wurde 30 Std nach Deiquat-Aufnahme durch Darmspülung 130mal mehr Deiquat entfernt als durch vollständige Aspiration des Mageninhaltes. In vitro-Versuche ergaben, daß bei Blutserumkonzentrationen von 1–2 ppm, die bei Vergiftungen oft gemessen werden, durch Hämodialyse keine toxikologisch relevanten Paraquat- oder Deiquat-Mengen entfernt werden können. Dagegen erwies sich die Hämodialyse bei 20 ppm und einer Blutumlaufgeschwindigkeit von 100 ml/min mit einer Clearance von 70 ml/min als wirksam. Die Hämoperfusion mit beschicheter Aktivkohle war in diesen Versuchen aber eindeutig überlegen, denn insbesondere bei Konzentrationen um 1–2 ppm waren die Clearance-Werte 5–7mal höher als bei der Hämodialyse.Die in vitro-Ergebnisse wurden bei einem Patienten mit einer Paraquat-Vergiftung bestätigt: Bei Konzentrationen unter 1 ppm war die Hämodialyse wirkungslos, während durch Hämoperfusion relativ hohe Clearance-Werte erreicht wurden, so daß der Serumspiegel rasch unter die Nachweisgrenze abfiel.

     

In vitro studies on sterically stabilized liposomes (SL) as enzyme carriers in organophosphorus (OP) antagonism

This study describes a new approach for organophosphorous (OP) antidotal treatment by encapsulating an OP hydrolyzing enzyme, OPA anhydrolase (OPAA), within sterically stabilized liposomes. The recombinant OPAA enzyme was derived from Alteromonas strain JD6. It has broad substrate specificity to a wide range of OP compounds: DFP and the nerve agents, soman and sarin. Liposomes encapsulating OPAA (SL)* were made by mechanical dispersion method. Hydrolysis of DFP by (SL)* was measured by following an increase of fluoride ion concentration using a fluoride ion selective electrode. OPAA entrapped in the carrier liposomes rapidly hydrolyze DFP, with the rate of DFP hydrolysis directly proportional to the amount of (SL)* added to the solution. Liposomal carriers containing no enzyme did not hydrolyze DFP. The reaction was linear and the rate of hydrolysis was first order in the substrate. This enzyme carrier system serves as a biodegradable protective environment for the recombinant OP-metabolizing enzyme, OPAA, resulting in prolongation of enzymatic concentration in the body. These studies suggest that the protection of OP intoxication can be strikingly enhanced by adding OPAA encapsulated within (SL)* to pralidoxime and atropine.     

Aquatic Insects and Trace Metals: Bioavailability,Bioaccumulation, and Toxicity

Abstract

The uptake of metals from food and water sources by insects is thought to be additive. For a given metal, the proportions taken up from water and food will depend both on the bioavailable concentration of the metal associated with each source and the mechanism and rate by which the metal enters the insect. Attempts to correlate insect trace metal concentrations with the trophic level of insects should be made with a knowledge of the feeding relationships of the individual taxa concerned. Pathways for the uptake of essential metals, such as copper and zinc, exist at the cellular level, and other nonessential metals, such as cadmium, also appear to enter via these routes. Within cells, trace metals can be bound to proteins or stored in granules. The internal distribution of metals among body tissues is very heterogeneous, and distribution patterns tend to be both metal and taxon specific. Trace metals associated with insects can be both bound on the surface of their chitinous exoskeleton and incorporated into body tissues. The quantities of trace meals accumulated by an individual reflect the net balance between the rate of metal influx from both dissolved and particulate sources and the rate of metal efflux from the organism. The toxicity of metals has been demonstrated at all levels of biological organization: cell, tissue, individual, population, and community. Much of the literature pertaining to the toxic effects of metals on aquatic insects is based on laboratory observations and, as such, it is difficult to extrapolate the data to insects in nature. The few experimental studies in nature suggest that trace metal contaminants can affect both the distribution and the abundance of aquatic insects. Insects have a largely unexploited potential as biomonitors of metal contamination in nature. A better understanding of the physico-chemical and biological mechanisms mediating trace metal bioavailability and exchange will facilitate the development of general predictive models relating trace metal concentrations in insects to those in their environment. Such models will facilitate the use of insects as contaminant biomonitors.     

Alzheimer’s disease – current trends in basic and clinical research. Highlights from the 16th ECNP

Advances in the molecular biological knowledge of neuronal nicotinic acetylcholine receptors (nAChRs) have led to a growing interest by the pharmaceutical industry in the development of novel compounds that selectively modulate nAChR function. The ability of (-)-nicotine, an activator of nAChRs, to enhance attentional aspects of cognition in animals and humans, to exert neuroprotective and anxiolytic-like effects, and presumably to mediate the negative correlation between smoking and Alzheimer's (and Parkinson's) Disease, has focused interest on the potential therapeutic utility of modulators of nAChR function for treatment of some of the deficits associated with these progressive, neurodegenerative conditions. Numerous compounds are known which activate nAChRs and which might serve as lead compounds toward the development of such agents. The pharmacologic diversity of neuronal nAChR subtypes suggests the possibility of developing selective compounds which would have more favourable side-effect profiles than existing agents. This broader class of agents, collectively called cholinergic channel modulators (ChCMs), is anticipated to encompass compounds which would have more favourable side-effect profiles than existing agents, which generally exhibit low selectivity. This selectivity may be achieved by preferentially activating some subtypes of nAChRs (i.e., Cholinergic Channel Activators, ChCAs) or inhibiting the function of other subtypes (Cholinergic Channel Inhibitors, ChCIs). An overview of the biology of nAChRs and the rationale for the use of ChCMs for the treatment of dementia related to neurodegenerative diseases are presented, followed by a discussion of lead compounds and compounds under consideration for clinical evaluation.     

Steroidal sapogenin contents in some domestic plants

In order to find out the values of the steroid resources for the future use. the compositions and contents of steroidal sapogenins from 13 domestic plants have been investigated. As a result,Dioscorea nipponica, D. quinqueloba andSmilax china were found to have large amount of diosgenin. And pennogenin inTrillium kamtschaticum andParis verticillata, yuccagenin inAllium fistulosum, hecogenin inAgave americana and neochlorogenin inSolanum nigum were appeared to be major steroidal sapogenins.     

Pharmacological treatment of COVID-19: an opinion paper

The precocity and efficacy of the vaccines developed so far against COVID-19 has been the most significant and saving advance against the pandemic. The development of vaccines has not prevented, during the whole period of the pandemic, the constant search for therapeutic medicines, both among existing drugs with different indications and in the development of new drugs. The Scientific Committee of the COVID-19 of the Illustrious College of Physicians of Madrid wanted to offer an early, simplified and critical approach to these new drugs, to new developments in immunotherapy and to what has been learned from the immune response modulators already known and which have proven effective against the virus, in order to help understand the current situation.